Apparatus for drowning nitrocellulose



g- 1950 J. D. PEARSON El'AL 5 7, 13

APPARATUS FOR BROWNING NITROCELLULOSE Original Filed July 23, 1943 4 Sheets-Sheet 1 IN V EN TORS. J 010V DONHLDSMV PE'AIZS'ON JrDONALD GEORGEASHCROFT AT TORNE' Y J.- D. PEARSON El AL 1 ,918

APPARATUS FOR DROWNING NITROCELLULOSE Aug. 8, 1950 7 Original Filed July 23, 1943 4 Sheets-Sheet 2 INVENTORS, J0li/VDONHLDJONPEHRSON &DON.4LD GEORGE'flS/f CROF1 ATTORNEY A118; 1950 J. D. PEARSON EIAL 2,517,918

APPARATUS FOR BROWNING NITROCELLULOSE Original Filed July 23, 1943 4 Sheets-Sheet 3 INVENTORS, JOIHVDOJMLDSONPEARSON arm/41.12 050mm qsilcfiofl' H 7' TORNE Y Aug. 8, 1950 J. D. PEARSON El AL I APPARATUS FOR BROWNING NITROCELLULOSE Original Filed July 23, 1943 4 Sheets-Sheet 4 INVENTORS, Jomvpomzwsow PEARSON m w W G m1 M. w D n m N v w T m Patented Aug. 8, 1950 arrmarus roa nnowmo mraocmunosa John Donaldson Pearson and Donald George Aalicroft, Saltcoata, Scotland, aaclgnora to Imperial Chemical Industries Limited, a corporation of Great Britain Original application m, as, 1943, Serial No.

11, 1945, Serial No. 821,689. In Great.

member 8, 1941 v 1,. This invention relates to the manufacture of nitrocellulose by processes in which the separation of the waste nitration acid fromthe nitrocellulose is eifected centrifugally, and relates more particularly'to processes, for the centrifugal separation of the waste acid in which 'specialprovision is made for the drowning of the centrifuged nitrocellulose; The invention is applicable to the separation of waste nitration acid from the nitrocellulose independently of the process by which nitration has been effected, and may be applied, for example, where the nitration has been effected by the so-calied mechanical and pot processes, and also where the nitration has itself bem conducted in a centrifuge. 1

This is a divisional application of application serial No. 495,884, filed July 23, 1943, which has become abandoned.

In processes of the aforementioned description it is frequently the custom to separate the nitro-.

cellulose from the waste acid in a centrifugal whereof the casing is provided with an outlet for the waste acid at its periphery and a basal outlet in the region of its axis leading to a drowning funnel, and the basket is provided with a similarly situated basal outletclosed by a removable cover. After the greater part of the waste acid has been removed by the rotation of the centrifugal basket, the rotation is discontinued and the cover is removed by the operator, who then breaks up the resulting annular cake of nitrocellulose moistwith waste acidand drops it in pertions into a funnel in which it is drowned in a large volume of cold water that has been caused to stream rapidly into the upper part ofthis funnel. The waste acid associated with the centrifuged nitrocellulose is thereby rapidly brought to a highly diluted state, and the drowned nitrocellulose falling from the funnel, if desired after further purification, The undiluted. waste acid that flows from the casing of the centrifugal is collected in a receptacle which is commonly made of mild steel, and is afterwards refortifled.

The nitration of cellulose is a reversible reaction, and denitration' proceeds with greatest velocity when the nitrocellulose is left in contact with an acid that is more dilute than the original waste acid, but less dilute than that presentinthe fully drowned mixture. It is well known is thereafter stabilised;

Divided and this application October Britain 5 Claims; (Cl. 210-41) that in the drowning operation the dilution of the waste acid associated with the centrifuged nitrocellulose must be rapidly effected in order to prevent the nitrogen content of the product being reduced appreciably and the product consequently being rendered useless or even decomposing violently.

The centrifuged cake of nitrocellulose moist with the undiluted waste acid is moreover very liable to fume off or fire with 'sumcient violence to injure the operator while he is dropping it into the drowning funnel. Such decompositions are especially violent and dangerous in the case of high nitrogen nitrocellulose such as guncotton. In the centrifuged cake of nitrocellulose conditions are favourable to the local development of high temperatures as a result of its being splashed with small quantities of water or other foreign material capable of diluting or chemically reacting with the waste acid associated with the nitrocellulose in the cake, and many of the dangerous decompositions that so frequently occur in practice may be attributed to splashes of water from the drowning funnel or other source finding their way into the centrifugal. Apart from dangerous manifestations, it is frequently found that in humid weather the nitrogen content of the nitrocellulose is sufllciently lowered to affect its solubility properties adversely, and this we attribute to the exposure of the cake of nitrocellulose to the atmosphere entailed while the operator is emptying the contents of the centrifugal basket into the drowning funnel.

It is an object of the present invention to provide an improved method and apparatus for the dilution of the waste acid associated with the centrifuged nitrocellulose cake, whereby the liability to the aforesaid hazards and disadvantages is reduced, and other advantages are attained.

According to the present invention, when the waste acid has ceased to drain from the annular cake of centrifuged nitrocellulose the liquid communication between the cake and the collected undiluted waste acid is cut, and thereafter the nitrocellulose is drowned while spinning by treating it with a stream of cold water, adequate to reduce its acidity to the desired value while effectively maintaining its nitrogen content, in the form of two or more equal curtains directed symmetrically with reference to the axis of rotation and distributed over the whole axial length of the annular. cake of nitrocellulose; thestream of drowning water is interrupted any residuum of the interrupted stream of drowning water in a position from which it can come into contact with a fresh charge in the centrifuge is displaced from said position with the aid of a medium indifferent to the undiluted waste acid; the said displaced water is removed from the centrifuge by spinning thereof; and thereafter communication with the collected undiluted waste acid is restored; the centrifuge being brought to rest at some stage in the sequence of operations after the stream of drowning water has been interrupted, the drowned charge then being removed from the centrifuge, and the centrifuge being thereafter recharged with nitrocellulose and waste acid or with cellulose and nitrating acid.

Since it is impracticable to interrupt the stream of drowning water at the locus where it is being distributed to the nitrocellulose, there will in practice be a residuum of the drowning water stream which must be removed so as to prevent it from finding its way into contact with the next batch of the mixture of nitrocellulose and waste acid or with the next nitration charge. The removal of this residuum may conveniently be eifected by displacing it forwardly with compressed air, or with waste acid or the like liquid substantially without heating effect.

It will be understood that in carrying out the present invention it is necessary strictly to observe the sequence of the following operations, namely spinning away the undiluted waste acid, cutting communication between the centrifuge and the waste acid receptacle, applying the drowning water, displacing residual drowning water, removing said residual drowning water from the centrifuge, re-establishing communication between the centrifuge and the waste acid receptacle. Within the framework of this sequence, however, certain variations may be made as to the time at which the centrifuge is brought to rest and the charge removed and the centrifuge recharged. Thus, after the stream of drowning water has been interrupted, we may discontinue spinning and remove the cake of nltrocellulose before displacement of the residual water, in which case the centrifuge may be restarted in order to remove the displaced water before the connection to the waste acid is reestablished and the new charge introduced. In this case we may use either compressed air or waste acid for displacing the residual drowning water. Preferably, the displacement of the residual drowning water may be carried out while the centrifuge is still spinning, although in this case it is necessary to use compressed air for the displacement, and in this alternative the residual drowning water after displacement is removed from the centrifuge through the cake of nitrocellulose, which is still in position, the centrifuge being thereafter brought to rest and the cake of nitrocellulose removed. 1

Variations may also be made in the time at which the centrifuge is recharged relative to the above-mentioned sequence of operations. Thus, spinning may be in progress before com munication with the waste acid receptacle is reestablished and a new charge introduced after such re-establishment of communication. A1- ternatively, communication may be re-established with the waste acid receptacle with the centrifuge at rest, and the new charge may be introduced either while the centrifuge is at rest or while the centrifuge is spinning, although desirably at a speed considerably below that employed during the drowning operation. Moreover, in the case where the nitration is conducted ln the centrifuge the new charge of acid may be introduced in part while the centrifuge is stationary, but the remainder of the acid together with the cellulose should be added after spinning has been recommenced and while the centrifuge is rotating slowly.

It is not essential that each individual curtain of drowning water should present an unbroken front along the axial length of the nitrocellulose cake over which it is distributed, provided that the water curtains are arranged so that every part of the exposed area of the rotating nitrocelluloselc'ake is impinged at least once in every rotation,' and that the balance of the apparatus is maintained. Thus for instance there may be used curtains consisting of successively staggered rows of jets so that the water is sprayed more or less evenly over the area of the nitrocellulose irrespective of its rotation, but it is quite sufilcient to use a single pair of diametrically oppositely directed curtains of water each unbroken over the whole axial length of the cake. It will be understood that while introducing the charge of the mixture of nitrocellulose and waste acid the rotation is desirably reduced to a speed considerably below that during the drowning operation or interrupted altogether.

The present invention also includes apparatus for the production of drowned nitrocellulose from the mixture obtained in the nitration of cellulose, comprising a centrifuge, means for introducing thereinto a charge of nitrocellulose and waste acid or a charge of cellulose and nitratin acid, one or more drowning water distributors each capable of directing a curtain of drowning water symmetrically with reference to the axis of rotation and distributed over the whole axial length of the filter element of the centrifuge, outlet control means comprising a two-way valve adapted to control the liquid communication between the centrifuge on the one hand, and either a spent drowning water sump or a waste acid receptacle on the other hand, means to control the supply of drowning water to the said distributors, and means to displace residual water from the distributors into the centrifuge when the supply of drowning water is cut off.

More particularly the apparatus according to the present invention comprises a drowning water valve, means to actuate a two-way valve to establish communication between the centrifugal and the spent drowning water sump and open the drowning water valve when such communication has been completely established, means to close the drowning water valve, and means operative on the closure of the drowning water valve first to displace the residual water and thereafter to actuate the two-way valve to establish communication between the centrifugal and the waste acid receptacle.

One suitable form of apparatus is illustrated for carrying out the process according to the invention in the accompanying drawings whereof Fig. 1 is a vertical section in a non-axial plane, and Fig. 2 is a plan view along the line ABCD in Fig. 1, both figures being of a portion of the apparatus showing the means whereby the curtains of drowning water are directed on to the nitrocellulose in the centrifugal: Figs. 3 and 4 are respectively a vertical section and a vertical side view showing the two-way valve by which the effluent. from the centrifugal is diverted away from the drowning water sump towards the undiluted waste acid receptacle and vice versa and the manner in which the drowning water supply :is controlled: and Fig. 5 is a vertical axial section of a modified form of the centrifuge portion of the apparatus in which the drowning of the nitrocellulose takes place.

InFig. l, I, 2 and 3 represent respectively the open mouthed basket with perforated walls, the casing and the driving shaft of the centrifugal. 24 is the extension of the driving shaft to which the basket is attached and it is in the form of a spider, 4 is an annular bell cover provided with a handle 4a resting on an upstand 23 boundin openings in .the base of the centrifugal basket near the driving shaft, through which the drowned nitrocellulose is dropped through an axial opening in the bottom of the centrifugal casing, the entrance to which is guarded by the flange 2a on the casing and the flange i2 on the basket. I is one of a number of ducts leadin through pipe II into the centrifugal basket from a number of cellulose nitration apparatus, two of these ducts being shown at 5 and 5' in'Fig. 2. 3 is the flanged outlet from the centrifugal casing 2 of which the base is slightly inclined towards it, I is a flanged pipe leading from the flanged outlet 3 to the two-way valve illustrated in Figs. 3 and 4. 3 is a lid on the centrifugal casing and 3 main self-closing drowning water supply valve and 43 the main drowning water supply pipe; 41, 41' are angled supports for air cylinder 33 and the water valve bracket 43 and are attached to the bracket 44 on the support 35. 43 is a piston valve and 43a its piston valve rod. 53 and 33a are arms attached to the piston rod II of the piston not shown in the cylinder 53 which operate rods 43a and 32 respectively. The piston rod 3i when it impinges a valve stem 53 opens the main water valve 45. In the supply air line I1 is valve 52 which is a self closing valve operated when the arm 50a impinges its valve stem 32. 54 is the piston of the cylinder 42, and 55, "at are branches of anoperating fluid line leading respectively to the cylinder 42 and the by-passpiston valve 43. 33 and 33a are branches of an operating fluid line respectively to the cylinder 53 and to the by-pass valve 43, from which latter the fluid line is continued as 33b into the top of the cylinder 42.

Beyond the piston valve 43 the line 55a is con tinued as line 55b to the cylinder 53. 51 is a gland through which thepiston rod 5| passes towards a drowning water valve stem 53; 33 is a bracket supporting the by-pass piston valve 43.

3 is a shaft guard, III is a hook on which the handle, 4a of the bell cover 4 is hung while the centrifugal is being emptied of drowned nitrocellulose. I 3 represents the floor of the building and I4 and Ma represent rising portions of a drowning water supply conduit leading from a main water valve 45 shown in Figs. 3 and 4. The angled upper portion No is flanged and bolted to another angled and descending portion I3 of the conduit leading directly through the centrifugal casing into the centrifugal basket and bolted to the centrifugal where the upper part of the pertion I3 passes through an extension I5 of the centrifugal casing. The lower end of the portion l3 of the conduit is connected through a Y tube l9 to two distributing tubes 23,23, one of which is shown broken oil in Fig. 1, to which are attached the distributing slot jets 2i and 2l, of which only one is shown in Fig 1. II is an air line, and I6 a non-return air valve controlling the supply of compressed air to an air injector 22 leading into the highest portion of the water supply conduit in the portion Ila.

In Figs. 3 and 4 the parts 3, I, I3, l4 and II have the same significance as in Fig. 1. The parts comprising the two-way valve are the casing 25, the cover plate 23, the ported plug 21, the valve stopper ring 23 and the valve rod 32 screwed into the ported plug 21. 23 is a bent outlet pipe provided with a housing 23a to accommodate a stufllng box 33 for the valve rod 32. 30 is a connecting pipe leading from the bent outlet pipe 29 to a sump for the spent drowning water, not shown. 3| is a connecting pipe leading to a waste acid receptacle not shown.

. 34 is the gland of the stufling box 33. 35, 35', 35"

are supporting rods, 33 is a save-all, and 31 a drain leading from it; 33 is an operating bar attached to valve rod 32; 33 is a knuckle joint attaching the end of the valve rod 32 to the piston rod 53 passing through the gland 43 of a cylinder 42, supported by the plate 4i. 43 is a self-closing by-pass piston valve housed on a supporting bracket 3|, and 43a is its piston valve rod operated by upward movement of bar 33. 45 is a In Figs. 3 and 4 the apparatus is illustrated with the valve in position to permit the waste acid to enter the waste acid receptacle and prevent it from contaminating the spent diiwnlng water in the sump.

In the operation of the valve operating gear the operating fluid is advantageously compressed air and the following description of its operation has reference to the use of that fluid. Compressed air is passed by the line 55 into the cylinder 42 whereby the piston 54 is driven upwards and the valve rod 32 attached by the knuckle joint 35 to the end of the piston rod 53 is caused to move the ported plug 21 upwards to the end of its stroke whereby the communication between the pipe I and the waste acid receptacle is cut off anda connection is opened between the pipe I and pipes 29 and 30. At the end of this upward stroke the operating bar 33 attached to the valve rod 32 strikes the piston valve rod 43a and thereby opens the bypass valve 43 and permits compressed air to pass from the line 55a to the line 55b and thence into the cylinder 53 at its outer end. The resulting motion of the piston rod 5| of that cylinder causes it to impinge the valve stem 53 and so open the self-closing drowning water valve 45. This allows water to pass from the inlet water pipe 46 t9 the portions i4, l4a and I3 of the drowing water supply conduit, and so through the Y tube and the distributing tubes 23 and 23' out of the slot jets 2i and 2| so as to drown the nitrocellulose in the rapidly spinning centrifugal basket. At this period of the operation the centrifuge is desirably rotating at full speed, and the water pressure should be suflicient to deliver something of the order of 10 to 20 times the weight of the nitrocellulose calculated on a dry basis in about one to two minutes. After the nitrocellulose has been thoroughly drowned, compressed air is allowed to pass by the line 56 into the inner end of the air cylinder 53 so as to drive back the piston rod an external line not shown through the air line H and the non-return valvei6 and so through the air injector 22 so as to forcibly displace any residual water between the injector 22 and the slot jets 2| and 2! into the still spinning centrifugal basket, from which the equivalent quantity of spent drowningwater passes into the pipes 8 and 1 and to the spent drowning water sump. As the piston rod terminates its stroke, the rigid arm 50 attached to it impinges the piston valve rod 48a and so opens the piston valve 45 which admits compressed air .from the line 58a into the line 56b and so to the top of the air cylinder 42, thus moving the valve rod 32 and ported plug 21 downwards to re-establish communication with the waste acid pipe 3i, and cutting off communication with the spent drowning water pipes 28 and 38. The operator then stops the rotation of the centrifugal, releases the pressure in line 56,..opens the lidv 8 and the bell cover 4 and hangs it up by means of the handle 4a on the hook I0. He then discharges the annular cake of damp nitrocellulose through the openings bounded by the upstand 23, thereafter replacing the bell cover 4 and the lid 8. A fresh charge of nitrocellulose and waste acid is then admitted through one of the pipes II and ducts 5 into the centrifugal basket while the latter is at rest or running at a relatively slow speed. The rotation of the centrifugal basket is then brought to high speed and when the flow of waste acid through the pipe 3| has ceased the cycle of operations described above is recommenced. The operating fluid may be water instead of air.

The nature of the apparatus used in carrying out the present invention is governed to a certain extent by the nature of the cellulose employed. Thus, cotton linters or wood pulp cellulose may be nitrated either by the pot process or by the mechanical process, and the products of the nitration may be transferred to an overhead driven centrifuge of the kind above described. Cotton cops are liable, however, to yield a tangled nitration product and are customarily nitrated by the pot process, and a product of this nature could not conveniently be handled in an overhead driven centrifuge of the kind above described, and it is more suitable to employ an under driven centrifuge from which the drowned nitrocellulose may be removed by hand from above. Either form of cotton may be nitrated directly in a centrifuge, but in this case again it is preferred to use an under driven centrifuge, owing to the weight of the nitration charge. A suitable form of under driven centrifuge in which it is possible to carry out the whole process of nitration, separation of waste acid and the drowning is illustrated in Fig. 5. This modified form is applicable to the case in which the nitration of the cellulose, as well as the drowning of the nitrocellulose, takes place in the basket of a centrifuge. It can also be used when the nitration is carried out outside the centrifuge and is better adapted than that illustrated in Fig. 1 and Fig. 2 of the drawings for the drowning of forms of nitrocellulose that are difllcult to pass through restricted apertures or passages, for instance nitrated cotton cops.

In Fig. 5 64 is the floor of a building, 65 is a supporting framework, 88 is a sloping base plate carried by the supporting framework, 18 is the outer vertical casing .of the centrifuge. 61 is the shaft of the centrifuge, 68 is a pulley and 69 is a driving belt. II is the perforated, centrifugal basket wall, and I2 is the basket hub member 8 y mounted to rotate withthe shaft '81. 18 is a retaining nut and a removable housing. 14 is the shaft housing and 15 represents the two hinged halves of a cover that is shaped tocover in the whole of the circular area in the-top of the casing 18 and also the housing 88, when they are closed, as shown by the broken lines. The solid lines indicate the opened position of the two halves of this cover. 18 is a retractable water spray distributing pipe that branches into two diametrically opposed nozzles 11 disposed within the basket clear of the basket hub member 12 and the housing 90. These nozzles have perforations arranged to permit the water to form curtains that are unbroken over the whole height of the rotating cake of nitrocellulose, shown at 18, where they impinge upon it at the diametrically opposite positions.

19 is a framework carrying a sleeve 80 through which the descending portion of the drowning water pipe 8| and the distributor 16 to which it leads can be caused, by means of a counterweighted cable 85, passing over a pulley not shown, to slide up and down to allow the distributing pipe and nozzles to be raised out of or lowered into the centrifuge. 82 and 83 are stops limiting the motion of the pipe 8|. 84 is a flexible connection leading to the pipe 8| which may be arranged to be fed from the drowning water supply pipe [4 shown in Fig. 4 of the drawings. Si is a flexible compressed air line forming a continuation of the pipe I! shown-in the said Fig. 4, 92 is a nonreturn air valve controlling the supply of compressed air to an air injector 93 leading into the highest portion of the drowning water pipe 8|. The solid lines indicate the lower of the two limiting positions of the parts I6, I1, 8|, 82, 84, SI, 92 and 93. The upper of the two limiting positions of the parts 16 and I1 is also indicated by broken lines.

85 is the common outlet for the waste acid and the spent drowning water and 81 is a cock leading to the flanged pipe I, as shown in Figs. 3 and 4 of the drawings. 88 is an acid inlet pipe used and 89 a fume pipe.

When the nitration of the cellulose is to be carried out in the centrifuge, the cock 8! is turned so as to close oil? the outlet 86 from the pipe 1, and the pipe BI, is at the limit of its upward travel, thus holding the distributing tube and nozzles completely out of the centrifuge. A portion of the charge of nitrating acid, which is previously brought to a predetermined suitable temperature, is run into the centrifuge through the pipe 88, and the basket of the centrifuge is caused to rotate at a slow speed if it has not already been started up before or during this addition. The charge of cellulose is now intro duced into the slowly rotating centrifuge basket while the remaining portion of the nitrating acid is run in. The hinged halves 15 of the cover are then closed down and the nitration reaction is allowed to proceed for the required length of time with the basket still rotating at slow speed. The cook 81 is then opened to permit the waste acid to enter the pipe 'I, which, during all these operations, is in communication with the waste acid receptacle through a two-way valve 28, as shown in Fig. 3 of the drawings. The basket is now caused to rotate at full speed in order to spin away as much of the waste acid as can conveniently be removed, and as a result a cake of nitrocellulose is formed on the wall of the basket. The centrifuge cover is next opened up and the nozzles 11 are lowered into the basket by allowing the pipe 8| to descend to the limit. of its travel. The mechanism illustrated in Fig. i of the drawings is now actuated by the operator so as to perform the successive functions of establishing communications between the pipe 1 and the spent drowning water receptacle, and turning on the drowning water supply. The drowning water coming through the pipes 84 and 8| into the distributing pipe 16 is sprayed through the nozzles 11, thus drowning the rapidly rotating nitrocellulose.

The operator thereafter actuates the mechanism illustrated in Fig. 4 of the drawings so as to carry out the successive operations of shutting off the drowning water supply, displacing the residual drowning water and re-establishing com- "munication with the waste acid receptacle. The

drive of the centrifuge is also discontinued. The clearance of the residual drowning water is effected by the admission of a blast of compressed air through the compressed air pipe l1 shown in the aforesaid Figs. 3 and 4 and its continuation 9i, the non-return valve 92 and the injector 93, into the pipe 8|. The operator times it so that, although the drive has been discontinued, the centrifuge is still spinning when the residuum of drowning water associated with the lower part of the pipe 8|, the distributing pipe 16 and noz- --zles I1 is expelled into the centrifuge, so that an equivalent amount of water is spun away from the nitrocellulose cake. The timing is also such that the re-establishment of the communication between the pipe I and the waste acid receptacle does not take place until this displaced water has substantially ceased to flow through the'pipe I.

The cable 85 is next manipulated to bring the pipe 8| to the upper limit of its travel and thus lift the distributing pipe 16 and nozzles 'l'l out of the centrifuge and when the basket has come to rest the cake of drowned nitrocellulose is unloaded by hand.

If the apparatus shown in Fig. is not to be used for nitration of the cellulose, as well as the drowning, the cook 81 is left open permanently, and the said inlet pipe 88 is not used.

It is therefore obvious that the apparatus may be modifled if desired by omitting the cock 8! and the inlet pipe 88; if desired the place of the latter may be taken by a chute or the like for facilitating the charging of the centrifuge with the mixture of nitrocellulose and waste acid.

The invention not only has the safety advantage that a fume-oil or flre is less likely to occur than is the case by the hitherto used method of drowning the nitrocellulose charge after the waste acid has been centrifuged away from it, but also the advantage that the nitrocellulose which the operator unloads according to the present invention is already drowned, so that he does not require to be in close proximity to the nitrocellulose when it is most liable to decomposition, and when it is least pleasant to handle on account of the fumes. The drowning operation is therefore a more pleasant and less hazardous task for the operator.

It will be understood that other forms of apparatus than that particularly described may be used for the purposes of the invention.

We claim:

1. Apparatus for the production of drowned nitrocellulose by a repeated batch process comprising a centrifuge having at least one inlet for nitrocellulose and acid, drowning water distributors within said centrifuge, said distributors having means for displacinglrgsidual water therein,

an outlet for said centrifuge, said outlet having a two-way valve connecting selectively with disposal means for said drowning water and receiving means for said waste acid, fluid operated means adapted for actuating said two-way valve for establishing communication between the centrifuge and the disposal means for said drowning water and thereafter for causing drowning water .to flow to said distributors, and a delay action fluid operated cylinder adapted first to terminate the flow of drowning water from said distributors, then to actuate the residual water displacing means and thereafter to cause said two-way valve to establish communication between said centrifuge and said. waste acid receiving means.

2. Apparatus for the production of drowned nitrocellulose by a repeated batch process as set forth in claim 1 wherein said drowning water distributors within said centrifuge are disposed symmetrically with reference to the axis of rotation of the same.

3. Apparatus for the production of drowned nitrocellulose by a repeated batch process comprising a centrifuge having at least one inlet for nitrocellulose and acid, drowning water distributors within said centrifuge, said distributors having means for displacing residual water therein, an outlet from said centrifuge provided with a. two-way valve connecting selectively with disposal means for said drowning water and receiving means for said waste acid, fluid operated means for said valve adapted upon establishing communication between said centrifuge and said drowning water receiving means to actuate a delay action fluid operated cylinder and thereby cause water to flow through said distributors, said fluid operated cylinder being adapted upon sufflcient drowning of said nitrocellulose to terminate the flow of drowning water, actuate said residual water displacing means, and thereafter cause said two-way valve to establish communication between said centrifuge and said waste acid receiving means.

4. Apparatus for the production of drowned nitrocellulose by a repeated batch process comprising a centrifuge having at least one inlet for nitrocellulose and acid, drowning water distributors within said centrifuge, said distributors having means for displacing residual water therein, an outlet from said centrifuge provided with a two-way valve connecting selectively with disposal means for said drowning water and receiving means for said waste acid, a fluid operated piston adapted for actuating said two-way valve, a first self-closing valve for supplying water to said distributors, a second self-closing valve for supplying air to said residual water displacing means, and a delay action fluid operated cylinder adapted upon the establishment of communication between said centrifuge and said drowning water receiving means to actuate said first selfclosing valve and thereby drown said nitrocellulose and then to permit the closing of said first valve and actuate said second self-closing valve to cause removal of said residual water and then to actuate said fluid operated means for said twoway valve and thereby establish communication between said centrifuge and said waste acid receiving means. i

5. Apparatus for the production of drowned nitrocellulose by a repeated batch process as set forth in claim 3 wherein said delay action fluid operated cylinder causes said two-way valve to establish communication between said centrifuge and said waste acid receiving means after drownins water has been removed from said nitrocellu- Number lose by said centrifuge in an amount equivalent 1,212,831

to said residual water in said distributors. 1,820,374 JOHN DONALDSON PEARSON. 2,223,683

DONALD GEORGE ASHCROFT. 5 2,244,652

2,310,862 REFERENCES CITED 2,328,256 The following references are of record in the 2334475 flle of this patent: 10

UNITED STATES PA'I'ENTB Number Number Name Date 10,747

1,146,445 Phillips July 13, 1915 Name Date Spelman Jan. 16, 1917 Carlson Aug. 25, 1931 Roberts Dec. 3, 1940 Kochii June 3, 1941 Nessler Feb. 9, 1943 Breckenbridge Aug. 31, 1943 Wales Jan. 13, 1948 FOREIGN PATENTB Country Date Great Britain of 1891 

1. APPARATUS FOR THE PRODUCTION OF DROWNED NITROCELLULOSE BY A REPEATED BATCH PROCESS COMPRISING A CENTRIFUGE HAVING AT LEAST ONE INLET FOR NITROCELLULOSE AND ACID, DROWNING WATER DISTRIBUTORS WITHIN SAID CENTRIFUGE, SAID DISTRIBUTORS HAVING MEANS FOR DISPLACING RESIDUAL WATER THEREIN, AN OUTLET FOR SAID CENTRIFUGE, SAID OUTLET HAVING A TWO-WAY VALVE CONNECTING SELECTIVELY WITH DISPOSAL MEANS FOR SAID DROWNING WATER AND RECEIVING MEANS FOR SAID WASTE ACID, FLUID OPERATED MEANS ADAPTED FOR ACTUATING SAID TWO-WAY VALVE FOR ESTABLISHING COMMUNICATION BETWEEN THE CENTRIFUGE AND THE DISPOSAL MEANS OF SAID DROWNING WATER AND THEREAFTER FOR CAUSING DROWNING WATER TO FLOW TO SAID DISTRIBUTORS, AND A DELAY ACTION FLUID OPERATED CYLINDER ADAPTED FIRST TO TERMINATE THE FLOW OF DROWNING WATER FROM SAID DISTRIBUTORS THEN TO ACTUATE THE RESIDUAL WATER DISPLACING MEANS AND THEREAFTER TO CAUSE SAID TWO-WAY VALVE TO ESTABLISH COMMUNICATION BETWEEN SAID CENTRIFUGE AND SAID WASTE ACID RECEIVING MEANS. 